Chemical-analysis apparatus and process



July 27 1926. 1,594,264

H. HOWARD CHEMICAL ANALYSIS APPARATUS AND PROCESS Filed March 1, 1924 4 Shets-Sheet .L

70 wer July 27 1926.

A H. HOWARDv CHEMICAL ANALYSIS APPARATUS AND Pnocss Filed March 1, 1924 4 Sheets-Sheet 2 July 27 1926.

H. HOWARD CHEMICAL ANALYSIS APPARATUS AND PROCESS Filed Marohl, 1924 4 Sheets-Sheet 5 NUN nuwnkot:

it may be oil the type involvingr the principles ci operation of the Wheatsto'ne bridge, so arranged that a tlow of electric current 'will cause e, deiiection of e gulvanonieter needle, which muy in the Well known inanner be arranged to indicate and record the deflection in any suitable units oi measure nient and to control u how of electric current to the regulator 12..

The anolyzer 1G illustrated in Figs 2, 3, Lland 5 has u suitable base 1d upon *which is supported a rectangular box and its rectangular Wing 16. Both the lao-L15 and the Wing 16 are provided with removable coversg lfhe'boii 15 is divided into three compartments 17, 18 and 19 by vertical partr tion Wells 2G and 21, the Wall 20 extending to the top ot the bor; and the Wall 21 ero tending upwardly to about the level oi the top of the Wing 16., The compartment 17 does not entend to the base 1d but is cut od and provided with semicylindrical bot tom, as is illustrated in Figs. 2 and 5f. rlhe shaft 22 is mounted with one end in the bearing nut 23 carried by one side Well. of the box 15 and extends over the top of the parti tion 21, through an opening in the partition 20, through e stud-ing box 2d carried by the opposite side vvall ci the bon 15, and to the drlviiig` motor and reducing gears 25. A constant level of oleuni to be tested or analyzed is meinteined in the compartment 17 by means of the supply pipe 8 and the ovenlovv pipe 25 and e conslnht level of testing acid is maintained in the compartment 18 v by the test acid supply 9 and the overflow pipe 27. The compartment 19 houses two troughs 28 and 29 for deliverin test acid and oleum supplied thereto by tie measuring apparatus now to be described to the analyzing apparatus housed in the Wing 16.

The test acid and oleuin measuring appa ratus comprises thertwo dippers 30 und 31 which communicate respectively with the two concentric tubular conduits 32 and 33, said dippers and conduits being mounted to rotate with the shaft 22s The dippers 3i) and 31 are mounted to dip into the acid held in the coin artments 1'? and 1S, respectively, and to oliver acid therefrom into the conduits 32 und 33, respectively, which in turn deliver into the troughs 29 and 28, respectively The dip er 30 is in the forni of a hollow cylinder c osed et one end.l The other end of the cylinder is open and communicates with en L-sheped canal in the block 3d.' 1' the side ot the dip er is afhlshuped notch or opening 35 for tie admission of acid es it dips into the body oi? acid maintained in the compartment 1i". The blccli: 311-, as stated, has un bshaped canal, one arm of which is coaxial with the shaft 22 and tubular conduit The other erin of the L-shaped canal entends at right angles to the shaft 22 and receives the open end of the dipper receso-i 30.. The bloei;L 341 also has a screw threaded opening cooxiel with end extending :trom that arm ci the lD-sheped canal which is cocviel with the shaft 22a rlhis opening engages a screv threaded portion of the 22 and serves to support the block 34: with. the flipper 30 ond the conduit 32 upon the shaftv 'lhe conduit 33 is mounted u' on end concentric with the conduit 32 und is closed at its`end opposite to the trough 28 where it engages the conduit 32. lt has a lateral opening` in which it receives the open end ot the dipper 31. The dipper 31 is similar in construction to the dipper 3@ described above.

The troughs 28 and 29 are carried in the compartment 19 by transverse supports 3G and 37 and are inclined to permit the iiow of acid to the analyzing apparatus in the Wing 16.

In the Wing 16 is a supporting structure in the form of a cylindrical receptacle 38 having projections 39 on its inside Wall forming e nest for the Dewar flash 4:0, a lateral outlet near its bottoni projecting through the Wall of the Wing and two similar projections 41 and 4-2 on its outer Wall provided with openin ls and set screws for receiving and supporting the tubular members 43 and 4:1-, which in turn support the acid receiving vessels 45 and 4d rllhe vessels 45 and 46 preferably' are made of glass and therefore are supported as described. Acid is delivered'from the troughs28 and 29 to the vessels 45 and 46, respectively, through the spouts 1'? and 48, respectively, and is delivered from the vessels 45 and 46 into the mixing tube 51 by the overflow spouts /1-9 and 5G. The mixture of acids formed in the mixing tube then iiowsiinto the Dewar flash 40.

The mixing" tube 51 in which the oleuin and test acid are mined and in which a considerable rise in temperature takes place preferably is made oigold., It is acylindricel tube having an enlarged mouth re ceiving the delivery ends of the spouts 49 and 50 and the lower end is shaped to it the bottom ci' the Devoir flesh upon which it rests. Near the bottom of the tube 51 is an opening 52 through which the mixed acid discharges into the ewar fiask. The'cover to the Wing- 16 has three openings 53, 54;- and 55, provided with stuiing boxes which support thermometers in the vessels 45 and d6 and the Dewar Hush 4:0.. These three thermometers are connected as indicated in Fig: 1 with the recorder 11. The analyzer, excepting of course the driving mechanism which is of the ordinary construction, and

the cover to the bon 15, the Dewar iieslr and the units comprising the perte d5., flo, 47, 48, 49 and 50, which preferably are made of glass, and the mixing tube which preferably is mede ci gold, are made of ucv suitable structural materiel. Steel is s satisJu lSO ` water.

ai anal oleum i instead above, the

Ais is stated in the article above referred tierences in the composition oit 'the oituin give comparatively large changes temperature of the reaction product.

in the "he method theetfore is very accurate, although course the composition ot the test acid 'fairly constant and its temperature must not cnange too rapidly because changes in the composition of the test acid as well as sudden changes in its temperature will produce corresponding changes, although relativ-ely small, in the results.

In the .foregoing description and in the appended claims reference is made to heat ot reaction, being understood that heat of reaction is intended to include not only the heat generated. or absorbed when true chemical reactions taire place, but also heat changes produced by hydrations and dehydrations, solution and precipitation, solidification and iiqueiaction, and in fact to all known henomena in which a heat change takes pace which bears a definite relation to the composition of the material involved.

l claim:

l. Chemical analysis apparatus comprising a reaction vessel, a source of supply of a material to be analyzed, a source of supply 'of a material capable when mixed with said material to be analyzed ot' producing a heat reaction, means for delivering measured quantities ont' said materials into the reaction vessel, and means comprising heat responsive elements 'for directly indicating a characteristic of the diiierence between the equalizing temperature of said materials and the temperature of the mixture thereof in said reaction vessel.

2. Chemical analysis apparatus comprising a source of supply of a material to be analyzed, a source ofsupply of a material capable when mixed with said material to be analyzed of producing a heat Ireaction, a temperature equalizer, means for delivering said materials from said sources of supply to said 'temperature equalizer, a reaction vessel, means tor delivering measured quantities of said material from said temperature equalizer to said reaction vessel, and means comprising heat responsive elements for directly indicating a characteristic of the difference between the temperature of one of said materials at a point between said temcerature equalizer and said .ieaction Kessel and the t ture or he mintuie ancient said reax with appaiatus tor the contin ation o .Y mical product by tue interaction nt least tw^ "e agents, said apparatus Lding a. rei chamber, 'te l lines for separately deuyering 'the into the reaction chamber, and means tor the pr duct ci reaction trom the reaction Chamb tor regulet "he rate et feed ofiV feed mes, sy y' l means tor regulating the rate of 1i c ising a .reaction vessel, means for delivering thereto measured quantities ci rrotluct and of a'nur-.terial adapter when m d t ercwith to heat reaction, n ig a heat-i Sil/l sive element tie vessel for inf icat c' by changes of temperature therein cnanges in a character c ot the product, and tuated by the last named .means ing said rate of `iced.

ln apparatus 'tor continuous formation of sulfuric acid including absorbing apparatus, feed lines for vfeeding absorbing acid and S03 respectively thereto, means :tor varying the rate of iiow in one o said iced lines and means for withdrawing the sulfuric acid pro-duct from the absorbing apparatus, the combination of a reaction vessel, a source oit supply ot liquid adapted when mixed with said sulfuric acid product to produce a heat reaction, means connected with the said withdrawing means and with the said source ot supply for delivering measured quantities of said sulfuric acid product and of the said liquid into the reaction vessel., means including a heat-responsive element in the said vessel for indicating by` changes of 'temperature in the vessel changes in the degree of concentration of said sulfuric acid product, and means actuated by the last .named means for actuating said varying means.

5. In a chemical analysis apparatus the combination of a reaction vessel, se arate reservoirs, means tor maintaining su stantially constant levels of liquids in said reservoirs, clippers mounted to move in fixed aths dipping into said reservoirs, means tor delivering liquids from said dippers into said reaction vessel, and means comprising heat responsive elements tor directly indicating a characteristic of the difference between the equalizing temperature of the liquids in said reservoirs and Vthe temperature of the mixture of liquids lin said reaction vessel.

6. ln chemical analysis apparatus a reaction vessel, separate reservoirs, means for maintaining supplies of liquids in said reservoirs, means for delivering liquid 'from each of said reservoirs at a constant rate into said reaction vessel and means comprising heat responsive elements for directly inmeans ac- `for vari uids in said reservoirs and the temperaturel of the mixture' of liquids in the reaction vessel. Y

7. In chemical analysis apparatus a source of supply of a material to be analyzed, a source of supply of a material capable when mixedwvith said material to be analyzed of producing a heatreaction, a temperature equalizer, means for delivering said materials from said soucres of supply to said equalizer, reservoirs, means for separately delivering said materials from said temperature equalizer to said reservoirs, a reaction vessel, means comprising dippers mounted to move in fixed paths dipping into said reservoirs for delivering said materials from said reservoirs into said `reaction vessel at constant rates, and means comprising temperature responsive elements for directly indicating a characteristic of the difference between the temperatureof the liquid in one of said reservoirs and the temperature of the mixture of liquids in said reaction vessel.

8. Process of controlling the production of l0 a chemical product which comprises supplying a raw material and forming said product in a continuous operation, causing a portion -at least of said product to undergo a phenomenon involving a spontaneous temperature change in the presence of aytemperature sensitive device, and causing the eli'ect upon said deviceto automatically control the supply of said raw material.

9. Process of controlling the production of a chemical product which comprises supplyingva raw material and forming said product in a continuous operation, causing a supply of said product immediately follow-l ing its formation to undergo a phenomenon involving a spontaneous temperature change in the presence of a temperature sensitive device, automatically indicating and recording the temperature effect upon said device, and

causing said effect to automatically control 50 the supply of saidy raw material.

In testimony whereof, I alix my signature.

HENRY HOWARD. 

